Solid titanic sulphate



Patented Mar. 22,1932

FRIEDRICH! 'RA's P ,OFLLEVERKUSEN. mm 2mm wmsi F iwmsnonr, enmmn I T SIGNORSTOfiIQG. FARBENINDUSTBIE sx'rmnensnrrscmmy or .FRANKIORT-ON- 4'rnn-maimennmmaooaromrronoremnmnx;

somi) TITANIC sumfiariai i j m b awl- 1 Miam -1am... as, 1929,.sr1a1K61350 921; and m eermai la ru 3,719 285] "The present invention relatesto the manu facture. of {solid water isoluble titanyl or titanium sulphates from their. concentrated solutions. I i

. In the manufacture of solid water soluble titanylor titanium sulphates, there is a-difficulty inasmuchasfon evaporating to dryness,the titanium sulphate solutions tend to be hydrolyzedpartially and therefore are no morecompletelysoluble afterwards.

The invention renders possible themanufacture ofsolid, water soluble titanyl-. and

titanium sulphates. In accordancewith the invention concentrated titanylor titanium sulphate solutions, said solutions containing generally in a liter about 100 to 500 grams of TiO are subjected in a finely divided forln to the action of a heated current of air of a temperature of-about'250 Cato about 350 C.,

for example, in a Biihler'or Krause dryer.

The apparatus for carrying out our. drying process is described in Ullmann, Encyklopadie der Technisohen Ch'emie, I. edition,

volume 8, pages 111-113. The solidifying volume 11, page 450 (Biihler-dryer) advantageously a dryer is used which is constructed as a spray-apparatus, for example the dryer of Krause comp are UllmanmEncya klop'adie der .Technischen Chemie, I. edition,

' anhydrous inorganic salts which are capable of absorbing wateran'd binding it as water of crystallization; for example, Na SO I K Al (SO MgSO or oxides formingsuch water soluble sulphates with the,

sulfuric acid present which are capable of absorbingwater and bindingit as water of crystallization, for example MgO and A1 0 The addition of a solidifying agent not only increases considerably the efficiency of the The quantity of the trated aqueous solution ofltitanyl sulphate dryer, but. also prevents the dried powder. r p 4 In the claims and the specification, the, term solid,water bindinga'gents designates the substances described'above; i

agglomeration :of

Instead of addingthesolidfwaterbinding r agents to'theliquidsfto 'be solidified, a super-. ficial' solidification can be efiected by' first drying the concentrated titanylor titanium sulphate'solutionsin a finely'divided form' by'means of air andithen mixing or grinding with fthe solid, waterbinding agent. Inthis mannera more or'lessgranular powder is does not agglomerate. I

produced, which even after prolonged storing solidifying agent to be added I may be varied within the widest limits, but generally an amount of about 3% toj5% calculated 'onthe amount ofthe-tita- ,nium sulphates is sufficient.

' The invention illustrated by the following examples, butit is notrestrictedthereto: V

. Emampl e J.1000 liter of a heated,conc'encontain'ing in a litre about 400 grams ofTiQ areatomizedand driedina Krause d ryer an air ourrenthaving atemperature ofabout The powderthus obtainable canfbeused directly or'is'intimately mixed with anhydrous sodium sulphate. I

Ewample" ae'ro 1000 liter of {the titanium,

Sulphate solution are added 30 kgs. ofanhys dro'us sodium sulphate, then the solution: is

atomized and dried in a Krausedryer b'yzan air current 300 G. a H

4 Example 3;1000 liter of a;ooncentrated' aqueous solution of titanium sulphate, containingiin a literabout450 grams are having a temperature fof about mixed while hotwith; 40 of magnesium oxide and dried in a Krausedryer at about. i.

300 'The powder produced canfif desired,.be. ground with a further solidifying agent, forexample, starch.- 1

The term-titanium sulphate infth'e claims designates the, titanium sulphate lwell as the titanyl sulphate? V .Wefcla'im: A

" 1. The process which comprisesiaddin'gto c0 titanium sulphatesolution containing in one i a concentrated titanium sulphate solution 3-5%,-calculated on the amount of the titanium sulphate used, of a solid, water binding agent and subjecting. the solution in a finely divided form to the action ofa heated current of air of atemperature of about 250 2. The process which comprises adding to a concentrated titanium sulphate solution 3 5%, calculated on the amount ofthe titanium sulphate used, of anhydrous sodium sulphate and subjecting the solution in a finely divided form to the action of a heated currentof airof a temperature of about 250- 350 'C'. 3. The process which comprises adding to a titanium sulphate solution containing in a liter about 400 to about 500 grains of titanium dioxide 35%, calculated on the amountof the titanium sulphate used, of a solid, water bind ing agent and subjecting the solution in a finely divided form to the action of a heated current of air of a temperature of about 250350 C.

4.1 The process which comprises adding to a titanium sulphate solution containing in a liter about 400 to about 500 grams of titanium dioxide 35%, calculated on the amount of the titanium sulphate used, of anhydrous sodium sulphate and subjecting the solution in a finely divided form to the action of a heated current of air of a temperature of about 250350" G. r V a 5. The process which comprises adding to a concentrated titanium sulphate solution 35%, calculated on the amount of the titasolution in a finely divided form to the action of a heated current of air of a temperature of about 250350 C.

9. The process which comprises adding to a titanium sulphate solution containing in one liter about 400 to about 500 grams of titanium dioxide, 3-57 calculated on the amount of the titanium sulphate used, of an organic substance of high molecular weight capable of forming colloidal solutions,and

subjecting the solution in a finely divided In testimony whereof we have hereunto set our hands.

FRIEDRICH RASPE. [13.5.] PAUL WEISE. [14. s]

nium sulphate used, of a porous inert insoluble substance, and subjecting the solution in a finely divided form to the action of a heated current of air of a temperature vof about 6; The process which comprises adding to I a concentrated titanium sulphate solution 3 5%, calculated on the amount of the titaniumsulphate used, of an organic substance 7 of high molecular weight capable of forming colloidal solutions, and subjecting the solution in a finely divided form to the action of a heated current of air of a temperature of about 25035,0 C. v

r 7. Theprocess which comprises adding to a concentrated titanium sulphate solution 35%, calculated on the amount of the titanium sulphate used, of an anhydrousinorganic salt which is capableoi absorbing water and binding it as water of crystallization, and subjecting the solution in a finely divided form to theaction of a heated current ofair of a temperatureof about 250350 C. 8. The process which comprises adding to a liter about 400 to about 500 grams of titanium dioxide, 35 calculated on the amount of the titanium sulphate used, of a porous .inert'insoluble substance, and subjecting the 

